Trans-bis­(3-tert-butyl­pyridine-κN)bis­(4-tert-butyl­pyridine-κN)bis­(thio­cyanato-κN)manganese(II)

Reinert, T.; Jess, I.; Näther, C.

doi:10.1107/S1600536812041128

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 11| November 2012| Page m1333

doi:10.1107/S1600536812041128

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Trans-bis(3-tert-butylpyridine-κN)bis(4-tert-butylpyridine-κN)bis(thiocyanato-κN)manganese(II)

Thorben Reinert,^a ^* Inke Jess ^a and Christian Näther ^a

^aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth Str. 2, D-24098 Kiel, Germany
^*Correspondence e-mail: treinert@ac.uni-kiel.de

(Received 26 September 2012; accepted 1 October 2012; online 6 October 2012)

The asymmetric unit of the title compound [Mn(NCS)₂(C₉H₁₃N)₄] consists of one Mn^II cation located on a center of inversion, one thiocyanato anion, one 3-tert-butylpyridine ligand and one 4-tert-butylpyridine ligand in general positions. The tert-butyl group of the 4-tert-butylpyridine ligand is disordered over two sets of sites in a 0.60:0.40 ratio. The Mn^II cation is coordinated by six N atoms of four tert-butylpyridine ligands and two N-bonded thiocyanato anions within a slightly distorted octahedral coordination environment.

Related literature

For related structures, see: Nassimbeni et al. (1990 ) (4-tert-butylpyridine only). For the background to this work, see: Boeckmann & Näther (2010 , 2011 ).

Experimental

Crystal data

[Mn(NCS)₂(C₉H₁₃N)₄]
M_r = 711.92
Triclinic, $[P \overline 1]$
a = 9.5921 (7) Å
b = 10.7253 (9) Å
c = 11.6286 (10) Å
α = 66.870 (9)°
β = 68.011 (9)°
γ = 76.359 (9)°
V = 1014.59 (17) Å³
Z = 1
Mo Kα radiation
μ = 0.46 mm⁻¹
T = 200 K
0.13 × 0.09 × 0.05 mm

Data collection

STOE IPDS-1 diffractometer
7271 measured reflections
3845 independent reflections
3017 reflections with I > 2σ(I)
R_int = 0.037

Refinement

R[F² > 2σ(F²)] = 0.049
wR(F²) = 0.128
S = 1.03
3845 reflections
241 parameters
3 restraints
H-atom parameters constrained
Δρ_max = 0.92 e Å⁻³
Δρ_min = −0.88 e Å⁻³

Data collection: X-AREA (Stoe, 2008 ); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812041128/im2404sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812041128/im2404Isup2.hkl

checkCIF report

Comment top

The structure determination of the title compound was performed as part of a project on the synthesis of new coordination polymers based on transition metal thiocyanates and the investigations of their magnetic behaviour (Boeckmann et al., 2010; Boeckmann et al., 2011). Within this project we have reacted manganese(II)thiocyanate monohydrate with 4-tert-butylpyridine in water, which resulted in the formation of crystals of the title compound by accident. Apparently, the 4-tert-butylpyridine was contaminated with 3-tert-butylpyridine to a degree that allowed the formation of a few single crystals of the title compound. It was on the other hand not possible to obtain phase pure crystalline powder samples. In the crystal structure Mn atoms are surrounded by six N atoms of four tert-butylpyridine ligands and two N-bonded thiocyanato anions in mutual trans orientation in a slightly distorted octahedral geometry (Fig. 1). Mn···N distances range from 2.180 (3) Å to 2.337 (2) Å. It is also worth mentioning that so far no other compound containing 3-tert-butylpyridine has been reported in the CSD.

Related literature top

For related structures see: Nassimbeni et al. (1990) (4-tert-butylpyridine only). For the background to this work see: Boeckmann et al. (2010, 2011).

Experimental top

The title compound was obtained accidently during the reaction of 28.4 mg Mn(NCS)₂ × H₂O (0.15 mmol) with 44.4 µL 4-tert-butylpyridine (0.30 mmol), obtained from Sigma Aldrich, in 1.50 ml water at RT in a closed 3 mL snap cap vial. After three weeks colourless needles of the title compound were obtained.

Computing details top

Data collection: X-AREA (Stoe, 2008); cell refinement: X-AREA (Stoe, 2008); data reduction: X-AREA (Stoe, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

Fig. 1. : Molecular structure of the title compund with displacement ellipsoids drawn at the 50% probability level (symmetry code: i = -x + 1, -y + 1, -z + 2). Disorder is shown as full and open bonds.

Trans-bis(3-tert-butylpyridine-κN)bis(4-tert-butylpyridine-κN)bis(thiocyanato-κN)manganese(II) top

Crystal data top

[Mn(NCS)₂(C₉H₁₃N)₄]	Z = 1
M_r = 711.92	F(000) = 379
Triclinic, P1	D_x = 1.165 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.5921 (7) Å	Cell parameters from 6934 reflections
b = 10.7253 (9) Å	θ = 1.9–28.2°
c = 11.6286 (10) Å	µ = 0.46 mm⁻¹
α = 66.870 (9)°	T = 200 K
β = 68.011 (9)°	Needle, colourless
γ = 76.359 (9)°	0.13 × 0.09 × 0.05 mm
V = 1014.59 (17) Å³

Data collection top

STOE IPDS-1 diffractometer	3017 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.037
Graphite monochromator	θ_max = 26.0°, θ_min = 2.5°
Phi scans	h = −11→11
7271 measured reflections	k = −13→12
3845 independent reflections	l = −14→14

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.128	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0656P)² + 0.489P] where P = (F_o² + 2F_c²)/3
3845 reflections	(Δ/σ)_max < 0.001
241 parameters	Δρ_max = 0.92 e Å⁻³
3 restraints	Δρ_min = −0.88 e Å⁻³

Crystal data top

[Mn(NCS)₂(C₉H₁₃N)₄]	γ = 76.359 (9)°
M_r = 711.92	V = 1014.59 (17) Å³
Triclinic, P1	Z = 1
a = 9.5921 (7) Å	Mo Kα radiation
b = 10.7253 (9) Å	µ = 0.46 mm⁻¹
c = 11.6286 (10) Å	T = 200 K
α = 66.870 (9)°	0.13 × 0.09 × 0.05 mm
β = 68.011 (9)°

Data collection top

STOE IPDS-1 diffractometer	3017 reflections with I > 2σ(I)
7271 measured reflections	R_int = 0.037
3845 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.049	3 restraints
wR(F²) = 0.128	H-atom parameters constrained
S = 1.03	Δρ_max = 0.92 e Å⁻³
3845 reflections	Δρ_min = −0.88 e Å⁻³
241 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mn1	0.5000	0.5000	1.0000	0.03151 (17)
N1	0.6416 (3)	0.6660 (2)	0.9167 (2)	0.0419 (5)
C1	0.6822 (3)	0.7724 (2)	0.8511 (2)	0.0383 (6)
S1	0.73642 (11)	0.92047 (9)	0.75445 (13)	0.0912 (4)
N11	0.3015 (2)	0.65601 (19)	0.94157 (18)	0.0352 (5)
C11	0.1639 (3)	0.6132 (3)	0.9872 (2)	0.0418 (6)
H11	0.1523	0.5200	1.0387	0.050*
C12	0.0397 (3)	0.6983 (3)	0.9625 (3)	0.0481 (7)
H12	−0.0555	0.6641	0.9950	0.058*
C13	0.0547 (3)	0.8350 (3)	0.8892 (3)	0.0433 (6)
H13	−0.0307	0.8950	0.8713	0.052*
C14	0.1938 (3)	0.8843 (2)	0.8421 (2)	0.0367 (5)
C15	0.3133 (3)	0.7888 (2)	0.8708 (2)	0.0370 (5)
H15	0.4103	0.8199	0.8380	0.044*
C16	0.2198 (3)	1.0344 (3)	0.7629 (3)	0.0493 (7)
C17	0.3273 (5)	1.0455 (4)	0.6249 (3)	0.0840 (13)
H17A	0.3451	1.1411	0.5740	0.126*
H17B	0.2825	1.0116	0.5811	0.126*
H17C	0.4235	0.9910	0.6310	0.126*
C18	0.0701 (4)	1.1229 (3)	0.7584 (4)	0.0711 (10)
H18A	0.0896	1.2182	0.7083	0.107*
H18B	0.0043	1.1149	0.8483	0.107*
H18C	0.0206	1.0922	0.7156	0.107*
C19	0.2930 (4)	1.0855 (3)	0.8312 (4)	0.0690 (10)
H19A	0.3097	1.1815	0.7815	0.103*
H19B	0.3899	1.0312	0.8346	0.103*
H19C	0.2258	1.0765	0.9210	0.103*
N21	0.5965 (2)	0.4594 (2)	0.80246 (18)	0.0363 (5)
C21	0.5945 (4)	0.3378 (3)	0.7974 (3)	0.0516 (7)
H21	0.5477	0.2697	0.8769	0.062*
C22	0.6561 (4)	0.3048 (3)	0.6840 (3)	0.0527 (8)
H22	0.6509	0.2160	0.6872	0.063*
C23	0.7253 (3)	0.3997 (2)	0.5657 (2)	0.0349 (5)
C24	0.7275 (4)	0.5254 (3)	0.5714 (2)	0.0540 (8)
H24	0.7735	0.5954	0.4934	0.065*
C25	0.6638 (4)	0.5507 (3)	0.6890 (2)	0.0512 (7)
H25	0.6684	0.6383	0.6888	0.061*
C26	0.7927 (3)	0.3670 (3)	0.4375 (2)	0.0448 (6)
C27	0.6680 (9)	0.3097 (12)	0.4244 (8)	0.100 (3)	0.60
H27A	0.6334	0.2307	0.5030	0.150*	0.60
H27B	0.7087	0.2819	0.3462	0.150*	0.60
H27C	0.5828	0.3802	0.4156	0.150*	0.60
C28	0.8526 (15)	0.4830 (7)	0.3205 (6)	0.113 (4)	0.60
H28A	0.8932	0.4547	0.2426	0.170*	0.60
H28B	0.9333	0.5145	0.3314	0.170*	0.60
H28C	0.7714	0.5572	0.3093	0.170*	0.60
C29	0.9189 (9)	0.2494 (8)	0.4536 (6)	0.084 (2)	0.60
H29A	0.8789	0.1724	0.5324	0.125*	0.60
H29B	1.0016	0.2798	0.4628	0.125*	0.60
H29C	0.9567	0.2210	0.3759	0.125*	0.60
C27'	0.7316 (12)	0.4873 (11)	0.3296 (8)	0.064 (3)	0.40
H27D	0.7487	0.5748	0.3277	0.096*	0.40
H27E	0.6231	0.4843	0.3513	0.096*	0.40
H27F	0.7852	0.4773	0.2431	0.096*	0.40
C28'	0.9667 (10)	0.3858 (13)	0.3845 (9)	0.079 (3)	0.40
H28D	0.9795	0.4746	0.3828	0.118*	0.40
H28E	1.0105	0.3812	0.2952	0.118*	0.40
H28F	1.0181	0.3132	0.4426	0.118*	0.40
C29'	0.769 (2)	0.2383 (12)	0.4445 (10)	0.116 (7)	0.40
H29D	0.8157	0.2285	0.3574	0.174*	0.40
H29E	0.6597	0.2319	0.4733	0.174*	0.40
H29F	0.8134	0.1657	0.5076	0.174*	0.40

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0411 (3)	0.0235 (3)	0.0266 (3)	−0.0085 (2)	−0.0061 (2)	−0.00652 (18)
N1	0.0488 (13)	0.0310 (11)	0.0420 (11)	−0.0114 (9)	−0.0091 (9)	−0.0093 (9)
C1	0.0349 (14)	0.0326 (13)	0.0469 (14)	−0.0053 (10)	−0.0150 (11)	−0.0099 (11)
S1	0.0620 (6)	0.0369 (4)	0.1414 (10)	−0.0216 (4)	−0.0427 (6)	0.0232 (5)
N11	0.0437 (12)	0.0289 (10)	0.0315 (10)	−0.0072 (9)	−0.0101 (8)	−0.0083 (8)
C11	0.0470 (15)	0.0324 (12)	0.0417 (13)	−0.0122 (11)	−0.0088 (11)	−0.0086 (10)
C12	0.0404 (15)	0.0459 (15)	0.0531 (15)	−0.0123 (12)	−0.0083 (12)	−0.0137 (12)
C13	0.0407 (15)	0.0400 (14)	0.0451 (14)	−0.0019 (11)	−0.0118 (11)	−0.0133 (11)
C14	0.0417 (14)	0.0324 (12)	0.0315 (11)	−0.0043 (10)	−0.0077 (10)	−0.0095 (9)
C15	0.0393 (14)	0.0326 (12)	0.0340 (12)	−0.0086 (10)	−0.0065 (10)	−0.0080 (9)
C16	0.0475 (16)	0.0301 (13)	0.0551 (16)	−0.0028 (11)	−0.0099 (13)	−0.0055 (11)
C17	0.109 (3)	0.0498 (19)	0.0509 (19)	−0.018 (2)	0.0052 (19)	0.0024 (15)
C18	0.066 (2)	0.0398 (16)	0.091 (2)	−0.0001 (15)	−0.0324 (19)	−0.0019 (16)
C19	0.062 (2)	0.0373 (16)	0.107 (3)	−0.0050 (14)	−0.0248 (19)	−0.0252 (17)
N21	0.0482 (13)	0.0308 (10)	0.0283 (9)	−0.0064 (9)	−0.0089 (8)	−0.0101 (8)
C21	0.078 (2)	0.0334 (13)	0.0322 (12)	−0.0183 (13)	0.0019 (12)	−0.0103 (10)
C22	0.079 (2)	0.0310 (13)	0.0393 (14)	−0.0149 (13)	−0.0011 (13)	−0.0138 (11)
C23	0.0412 (14)	0.0330 (12)	0.0311 (11)	−0.0033 (10)	−0.0115 (10)	−0.0116 (9)
C24	0.086 (2)	0.0397 (14)	0.0294 (12)	−0.0248 (14)	−0.0041 (13)	−0.0078 (11)
C25	0.084 (2)	0.0333 (13)	0.0350 (13)	−0.0208 (13)	−0.0081 (13)	−0.0116 (11)
C26	0.0581 (17)	0.0444 (14)	0.0312 (12)	−0.0050 (12)	−0.0094 (11)	−0.0166 (11)
C27	0.078 (5)	0.181 (10)	0.091 (5)	−0.010 (5)	−0.023 (4)	−0.102 (7)
C28	0.221 (12)	0.065 (4)	0.027 (3)	−0.048 (6)	0.011 (5)	−0.017 (3)
C29	0.082 (5)	0.098 (5)	0.063 (4)	0.024 (4)	−0.012 (3)	−0.048 (4)
C27'	0.079 (6)	0.082 (6)	0.036 (4)	−0.001 (5)	−0.020 (4)	−0.027 (4)
C28'	0.056 (5)	0.114 (8)	0.057 (5)	0.015 (5)	−0.006 (4)	−0.044 (6)
C29'	0.205 (17)	0.079 (7)	0.052 (6)	−0.083 (10)	0.040 (8)	−0.047 (6)

Geometric parameters (Å, º) top

Mn1—N1	2.180 (2)	C21—C22	1.378 (4)
Mn1—N1ⁱ	2.180 (2)	C21—H21	0.9500
Mn1—N21	2.3081 (18)	C22—C23	1.380 (3)
Mn1—N21ⁱ	2.3081 (18)	C22—H22	0.9500
Mn1—N11ⁱ	2.337 (2)	C23—C24	1.381 (4)
Mn1—N11	2.337 (2)	C23—C26	1.531 (3)
N1—C1	1.157 (3)	C24—C25	1.380 (4)
C1—S1	1.614 (3)	C24—H24	0.9500
N11—C11	1.343 (3)	C25—H25	0.9500
N11—C15	1.344 (3)	C26—C29'	1.419 (9)
C11—C12	1.368 (4)	C26—C28	1.467 (7)
C11—H11	0.9500	C26—C29	1.534 (7)
C12—C13	1.387 (4)	C26—C27	1.546 (8)
C12—H12	0.9500	C26—C28'	1.580 (10)
C13—C14	1.385 (4)	C26—C27'	1.583 (9)
C13—H13	0.9500	C27—H27A	0.9800
C14—C15	1.393 (4)	C27—H27B	0.9800
C14—C16	1.535 (3)	C27—H27C	0.9800
C15—H15	0.9500	C28—H28A	0.9800
C16—C17	1.524 (4)	C28—H28B	0.9800
C16—C18	1.530 (4)	C28—H28C	0.9800
C16—C19	1.537 (5)	C29—H29A	0.9800
C17—H17A	0.9800	C29—H29B	0.9800
C17—H17B	0.9800	C29—H29C	0.9800
C17—H17C	0.9800	C27'—H27D	0.9800
C18—H18A	0.9800	C27'—H27E	0.9800
C18—H18B	0.9800	C27'—H27F	0.9800
C18—H18C	0.9800	C28'—H28D	0.9800
C19—H19A	0.9800	C28'—H28E	0.9800
C19—H19B	0.9800	C28'—H28F	0.9800
C19—H19C	0.9800	C29'—H29D	0.9800
N21—C25	1.327 (3)	C29'—H29E	0.9800
N21—C21	1.333 (3)	C29'—H29F	0.9800

N1—Mn1—N1ⁱ	180.000 (1)	C23—C22—H22	119.8
N1—Mn1—N21	89.88 (8)	C22—C23—C24	115.3 (2)
N1ⁱ—Mn1—N21	90.12 (8)	C22—C23—C26	121.8 (2)
N1—Mn1—N21ⁱ	90.12 (8)	C24—C23—C26	122.9 (2)
N1ⁱ—Mn1—N21ⁱ	89.88 (8)	C25—C24—C23	120.9 (2)
N21—Mn1—N21ⁱ	180.000 (1)	C25—C24—H24	119.6
N1—Mn1—N11ⁱ	90.23 (8)	C23—C24—H24	119.6
N1ⁱ—Mn1—N11ⁱ	89.77 (8)	N21—C25—C24	123.6 (2)
N21—Mn1—N11ⁱ	86.16 (7)	N21—C25—H25	118.2
N21ⁱ—Mn1—N11ⁱ	93.84 (7)	C24—C25—H25	118.2
N1—Mn1—N11	89.77 (8)	C29'—C26—C28	128.7 (5)
N1ⁱ—Mn1—N11	90.23 (8)	C29'—C26—C23	116.5 (4)
N21—Mn1—N11	93.84 (7)	C28—C26—C23	114.0 (3)
N21ⁱ—Mn1—N11	86.16 (7)	C29'—C26—C29	61.8 (8)
N11ⁱ—Mn1—N11	180.00 (10)	C28—C26—C29	109.6 (6)
C1—N1—Mn1	157.6 (2)	C23—C26—C29	108.3 (3)
N1—C1—S1	177.4 (2)	C29'—C26—C27	44.1 (8)
C11—N11—C15	117.1 (2)	C28—C26—C27	111.9 (6)
C11—N11—Mn1	118.51 (16)	C23—C26—C27	106.9 (3)
C15—N11—Mn1	124.28 (17)	C29—C26—C27	105.7 (5)
N11—C11—C12	122.7 (2)	C29'—C26—C28'	111.6 (8)
N11—C11—H11	118.7	C28—C26—C28'	59.6 (6)
C12—C11—H11	118.7	C23—C26—C28'	107.0 (4)
C11—C12—C13	119.2 (3)	C29—C26—C28'	55.6 (5)
C11—C12—H12	120.4	C27—C26—C28'	145.3 (5)
C13—C12—H12	120.4	C29'—C26—C27'	111.2 (8)
C14—C13—C12	120.2 (3)	C28—C26—C27'	42.7 (5)
C14—C13—H13	119.9	C23—C26—C27'	107.4 (4)
C12—C13—H13	119.9	C29—C26—C27'	142.3 (4)
C13—C14—C15	116.1 (2)	C27—C26—C27'	74.8 (6)
C13—C14—C16	123.6 (2)	C28'—C26—C27'	102.1 (6)
C15—C14—C16	120.3 (2)	C26—C27—H27A	109.5
N11—C15—C14	124.7 (2)	C26—C27—H27B	109.5
N11—C15—H15	117.6	H27A—C27—H27B	109.5
C14—C15—H15	117.6	C26—C27—H27C	109.5
C17—C16—C18	111.4 (3)	H27A—C27—H27C	109.5
C17—C16—C14	109.0 (2)	H27B—C27—H27C	109.5
C18—C16—C14	111.0 (2)	C26—C28—H28A	109.5
C17—C16—C19	108.8 (3)	C26—C28—H28B	109.5
C18—C16—C19	107.7 (3)	H28A—C28—H28B	109.5
C14—C16—C19	108.8 (2)	C26—C28—H28C	109.5
C16—C17—H17A	109.5	H28A—C28—H28C	109.5
C16—C17—H17B	109.5	H28B—C28—H28C	109.5
H17A—C17—H17B	109.5	C26—C29—H29A	109.5
C16—C17—H17C	109.5	C26—C29—H29B	109.5
H17A—C17—H17C	109.5	H29A—C29—H29B	109.5
H17B—C17—H17C	109.5	C26—C29—H29C	109.5
C16—C18—H18A	109.5	H29A—C29—H29C	109.5
C16—C18—H18B	109.5	H29B—C29—H29C	109.5
H18A—C18—H18B	109.5	C26—C27'—H27D	109.5
C16—C18—H18C	109.5	C26—C27'—H27E	109.5
H18A—C18—H18C	109.5	H27D—C27'—H27E	109.5
H18B—C18—H18C	109.5	C26—C27'—H27F	109.5
C16—C19—H19A	109.5	H27D—C27'—H27F	109.5
C16—C19—H19B	109.5	H27E—C27'—H27F	109.5
H19A—C19—H19B	109.5	C26—C28'—H28D	109.5
C16—C19—H19C	109.5	C26—C28'—H28E	109.5
H19A—C19—H19C	109.5	H28D—C28'—H28E	109.5
H19B—C19—H19C	109.5	C26—C28'—H28F	109.5
C25—N21—C21	115.7 (2)	H28D—C28'—H28F	109.5
C25—N21—Mn1	123.21 (16)	H28E—C28'—H28F	109.5
C21—N21—Mn1	121.01 (15)	C26—C29'—H29D	109.5
N21—C21—C22	124.0 (2)	C26—C29'—H29E	109.5
N21—C21—H21	118.0	H29D—C29'—H29E	109.5
C22—C21—H21	118.0	C26—C29'—H29F	109.5
C21—C22—C23	120.5 (2)	H29D—C29'—H29F	109.5
C21—C22—H22	119.8	H29E—C29'—H29F	109.5

Symmetry code: (i) −x+1, −y+1, −z+2.

Experimental details

Crystal data
Chemical formula	[Mn(NCS)₂(C₉H₁₃N)₄]
M_r	711.92
Crystal system, space group	Triclinic, P1
Temperature (K)	200
a, b, c (Å)	9.5921 (7), 10.7253 (9), 11.6286 (10)
α, β, γ (°)	66.870 (9), 68.011 (9), 76.359 (9)
V (Å³)	1014.59 (17)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	0.46
Crystal size (mm)	0.13 × 0.09 × 0.05

Data collection
Diffractometer	STOE IPDS1 diffractometer
Absorption correction	–
No. of measured, independent and observed [I > 2σ(I)] reflections	7271, 3845, 3017
R_int	0.037
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.049, 0.128, 1.03
No. of reflections	3845
No. of parameters	241
No. of restraints	3
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.92, −0.88

Computer programs: X-AREA (Stoe, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011), publCIF (Westrip, 2010).

Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. NA 720/3–1) and the State of Schleswig–Holstein. We thank Professor Dr Wolfgang Bensch for the opportunity to use his experimental facility.

References

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